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The resulting isotherms for the TiO2 fraction of the composite clearly display the hysteresis loops characteristic for a disordered mesopore system with a broad width distribution (Figure 2d). The pore size range of the TiO2 material increases with increasing mass fraction of TiO2 in the composite pointing at pore space between TiO2 particles formed during the sol-gel synthesis. Clearly, however, the presence of the zeolite affects the textural properties of the TiO2 formed, since the mesopores in the TiO2 prepared in the absence of the zeolites are much smaller, i.e., the hysteresis loop occurs at lower relative pressures (0.4–0.6, Figure 2d). It is, therefore, obvious that the TiO2 from sol-gel synthesis strongly interacts with the outer surface of the ZSM-5 zeolite crystals, although this interaction is expectedly reduced at higher TiO2 mass fractions. Details of the textural properties (specific surface area, pore volume, and average pore diameter) are shown in Table S1. The morphology and the proximity of the TiO2 particles and the crystals of zeolite ZSM-5 were further characterized by scanning electron microscopy (SEM) (Figure 3). The SEM images of the pure TiO2 from sol-gel synthesis and Hombikat show a broad particle size distribution, while Hombikat possesses somewhat more regularly shaped particles with sizes below 1 μm (Figure 3a,b). The crystallites of zeolite ZSM-5 are between 3 and 8 μm in diameter and partly intertwined (Figure 3d). These crystals are clearly visible in the composites from mechanical mixing (HZMM (50/50), Figure 3d) and from solid-state dispersion (HZSSD (50/50), Figure 3e). The TiO2 particles are aggregated and loosely packed around the ZSM-5 crystallites. In complete agreement with results from XRD and N2 sorption, there is no apparent difference in the composites obtained by mechanically mixing or by solid-state dispersion. In sharp contrast, however, greater surface of the zeolite crystals is covered with small TiO2 particles when prepared by sol-gel synthesis (TZSG, Figure 3f). Although larger TiO2 particles and agglomerates of around 2–5 μm diameter are also seen in the SEM image, the TiO2 particles are more evenly distributed over the zeolite surface and support the more intense and direct interaction between both components of the composites as already concluded from N2 sorption analysis (vide supra). Nevertheless, the contact between the TiO2 particles and the zeolite does not lead to a blockage of access to the zeolite pores as shown by the results from N2 sorption discussed above. Diffuse reflectance UV-Vis absorption spectra of TiO2 from sol-gel synthesis, Hombikat, and the composites TZSG (50/50), HZSSD (50/50), and HZMM (50/50) are shown in Figure 4. It can be clearly seen that all materials absorb light in the UV region with only small differences between the pure TiO2 samples and the TiO2/ZSM-5 composites as well the different preparation methods. This indicates that the preparation techniques and the presence of ZSM-5 have only a minor effect on the optical absorption of the TiO2 component in the composites. Nevertheless, a measurable blue shift of the absorption band edge of TiO2 and TZSG (50/50) from 160PDF Image | Zeolite Catalysis
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